CN105106151B - A kind of tablet for curing fracture and preparation method thereof - Google Patents
A kind of tablet for curing fracture and preparation method thereof Download PDFInfo
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- 208000010392 Bone Fractures Diseases 0.000 title claims abstract description 21
- 206010017076 Fracture Diseases 0.000 title claims abstract description 21
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Abstract
The invention discloses a kind of preparation method of tablet for curing fracture and its obtained product, and, using Ligusticum wallichii, aconiti preparata,radix, Radix Angelicae Sinensis, vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, pyritum ignited, No. four copper powders as raw material, its preparation method is for it：1）Take vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, the Radix Angelicae Sinensis extraction volatile oil in prescription；2）Ligusticum wallichii, aconiti preparata,radix, pyritum ignited, No. four copper powders in prescription are extracted with the above-mentioned dregs of a decoction using the method for continuous dynamic concentration of alcohol extraction；3) vacuum-concentrcted technique concentrated extracting solution is used；4）Above-mentioned medicinal extract, volatile oil are well mixed with proper auxiliary materials, particle is made, through softwood processed, pelletizes, dries, tabletting.Present invention improves over former preparation method, under conditions of more extracts active ingredients, strengthens active constituent content, and the dissolution of tablet is good, and bioavailability is high, evident in efficacy.
Description
Technical field:
The present invention relates to technical field of traditional Chinese medicine preparation, is specifically related to a kind of with the scattered stasis of blood, promoting blood circulation, the synthetism of analgesic effect
Piece and preparation method thereof.
Technical background：
Fracture is the most common traumatic illness of Orthopeadic Surgery clinic.Because the normal healing journey of bone needs the long period, sternly
Ghost image rings the live and work of patient.Therefore, the emphasis that union is always orthopaedics research how is rapidly promoted, tablet for curing fracture is
One kind is made up of Ligusticum wallichii, aconiti preparata,radix, Radix Angelicae Sinensis, vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, pyritum ignited, No. four taste drug matchings of copper powder 7, often
For wound and the Chinese patent drug of orthopaedics.With the scattered stasis of blood, promoting blood circulation, analgesic effect, it is mainly used in traumatic injury, injury of tendon and muscle fracture, extravasated blood
Swelling and pain etc..
The preparation method of second tablet for curing fracture of the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation：Above seven flavor medicine, No. four copper powders,
Aconiti preparata,radix, vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, pyritum ignited are ground into fine powder, sieve, and mix；Ligusticum wallichii, Radix Angelicae Sinensis are shone under liquid extract item
Percolation with 70% ethanol as solvent, be percolated, filtrate recycling ethanol, be concentrated under reduced pressure into cream, add above-mentioned fine powder and auxiliary
Material, mix, particle is made, less than 60 DEG C dryings, is pressed into 1000, sugar coating, produces.The preparation technology simple coarse, contains
Impurity is more, and effective component extraction rate is low, and action effect is not good enough.
Chinese patent application 201210388907.0 provides a kind of preparation method of new tablet for curing fracture, Ligusticum wallichii, Radix Angelicae Sinensis, vinegar
Stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar use supercritical CO2Abstraction technique is extracted, and aconiti preparata,radix, pyritum ignited use microwave-assisted extraction technique
To be extracted, the recovery rate of forulic acid significantly improves in this method, and still, this method has no the raising of other active ingredients, and
And Microwave Extraction is extracted using isoconcentration ethanol, recovery rate is still limited.
Secondly, clinically remain at present and play the problems such as time is slow, and product appearance is poor, ineffective in poor taste, drug effect.
In view of the above problems, it is special to propose the present invention.
The content of the invention
The main object of the present invention is to provide a kind of preparation method of tablet for curing fracture.This method can strengthen more active ingredients
Content, remove influence main ingredient composition impurity, improve the drug effect of tablet, while strengthen the quality controllability of tablet.
Preparation method：
(1) extraction of volatile oil
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder after mixing, cross 40 mesh sieves, first
Secondary plus bulk drug weight 0.5% cellulase and pectase (1.5:1), stir, add 6-10 times of water, keeping temperature
At 40 DEG C -60 DEG C, PH 4.0-5.5, after carrying out enzymolysis processing 1h, 0.7% cellulase and the fruit of bulk drug weight are added
Glue enzyme (1.5:1), then after digesting 1h it is put into water distillation apparatus device, carries out steam distillation extraction 4-6h, collect volatile oil；
(2) continuous dynamic concentration of alcohol extraction
The Ligusticum wallichii of recipe quantity, aconiti preparata,radix, pyritum ignited, No. four copper powders are ground into coarse powder to mix, cross 40 mesh scalpings, are merged
The dregs of a decoction in step (1), material is put into from the dog-house of extractor, and after feeding intake, 95% is added in Chinese medicament extracting device
Ethanol solution, to extractor carry out heating stirring, and control final temperature be 60 DEG C -75 DEG C；One water of connection at the top of extractor
Case, it is allowed to connect with extractor, valve switch and flowmeter is provided between water tank and extractor, wherein flowmeter can controls water
Water flows into the speed of extractor in case；While being heated to extractor, also water in water tank is heated, made in water tank
Water temperature is consistent with temperature in extractor；
After temperature stabilization in water tank and extractor, the valve switch of water tank is opened, water velocity is adjusted, makes concentration of alcohol
Rate of change is 0.75%-0.9%/min, reacts 50min-60min, after first set reaction terminates, collects extract solution；For the first time
The step of reacting the ethanol of addition 50% in the dregs of a decoction after terminating, and being reacted according to first slowly adds water, changes concentration of alcohol
Rate is 0.4%-0.5%/min, reacts 80min-100min；Filtrate is collected, is closed after cold filtration with the filtrate that first time collects
And obtain extract solution；
(3) vacuum-concentrcted
Relative density is 1.25- when using the vacuum-concentrcted technique to be condensed into 60 DEG C the extract solution in step (2)
1.26 thick paste, 60 DEG C be dried under reduced pressure after be ground into dry extract, cross 14 mesh sieves；
(4) preparation of tablet
Dry extract and volatile oil obtained above are taken, adds appropriate talcum powder and microcrystalline cellulose (2:1), carboxymethyl forms sediment
Powder sodium, it is well mixed, through softwood processed, pelletizes, dry, is pressed into 400, film coating, every 0.62g.
The present invention's has the beneficial effect that：
1st, vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis are first extracted volatile oil by the present invention, and the dregs of a decoction further use continuous dynamic second
Determining alcohol extracts, and can make full use of its more active component, and go out using enzymolysis pre-treatment extraction volatile oil, volatile oil
Oil cut rate is high.
2nd, Ligusticum wallichii, aconiti preparata,radix, pyritum ignited active ingredient extraction in, pass through continuous dynamic concentration of alcohol extract method
Rather than water decoction extraction method, the opposed polarity active ingredient in medicinal material can be fully extracted, while make active ingredient in decoction
Content significantly improve.
3rd, the time is reduced using being concentrated under reduced pressure in the concentration process of extract solution, prevents active ingredient heated quilt for a long time
Destroy.
4th, using tablet for curing fracture made from the preparation method described in step of the present invention (4), the medicine disintegration time limit is shortened, is improved
The bioavilability of product of the present invention.
5th, it is demonstrated experimentally that product of the present invention is because the recovery rate of effective ingredient is high, and in extract solution impurity content compared with
It is low, compared with traditional handicraft, drug effect enhancing.
Embodiment：
Embodiment 1
Preparation method：
(1) extraction of volatile oil
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder after mixing, cross 40 mesh sieves, first
Secondary plus bulk drug weight 0.5% cellulase and pectase (1.5:1), stir, add 6 times of water, maintain the temperature at
40 DEG C, PH 4.0, after carrying out enzymolysis processing 1h, add 0.7% cellulase and pectase (1.5 of bulk drug weight:1),
It is put into after digesting 1h again in water distillation apparatus device, carries out steam distillation extraction 5h, collect volatile oil；
(2) continuous dynamic concentration of alcohol extraction
The Ligusticum wallichii of recipe quantity, aconiti preparata,radix, pyritum ignited, No. four copper powders are ground into coarse powder to mix, cross 40 mesh scalpings, are merged
The dregs of a decoction in step (1), material is put into from the dog-house of extractor, and after feeding intake, 3 times of amounts are added in Chinese medicament extracting device
95% ethanol solution, heating stirring is carried out to extractor, and it is 75 DEG C to control final temperature；One water of connection at the top of extractor
Case, it is allowed to connect with extractor, valve switch and flowmeter is provided between water tank and extractor, wherein flowmeter can controls water
Water flows into the speed of extractor in case；While being heated to extractor, also water in water tank is heated, made in water tank
Water temperature is consistent with temperature in extractor；
After temperature stabilization in water tank and extractor, the valve switch of water tank is opened, water velocity is adjusted, makes ethanol dense
Degree rate of change is 0.75%/min, reacts 60min, concentration of alcohol is reached 50%, after first set reaction terminates, and collects extraction
Liquid；The step of ethanol that 4 times of amount concentration are 50% is added in the dregs of a decoction after first set reaction terminates, and is reacted according to first is delayed
Slow plus water, it is 0.5%/min to make concentration of alcohol rate of change, reacts 80min, concentration of alcohol is reached 10%；Collect filtrate, cooling
The filtrate collected after filtering with first time merges, and obtains extract solution；
(3) vacuum-concentrcted
When using the vacuum-concentrcted technique to be condensed into 60 DEG C the extract solution in step (2) relative density for 1.25 it is thick
Cream, 60 DEG C be dried under reduced pressure after be ground into dry extract, cross 14 mesh sieves；
(4) preparation of tablet
Dry extract and volatile oil obtained above are taken, adds appropriate talcum powder and microcrystalline cellulose (2:1), carboxymethyl forms sediment
Powder sodium, it is well mixed, through softwood processed, pelletizes, dry, is pressed into 400, film coating, every 0.62g.
Embodiment 2
Preparation method：
(1) extraction of volatile oil
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder after mixing, cross 40 mesh sieves, first
Secondary plus bulk drug weight 0.5% cellulase and pectase (1.5:1), stir, add 8 times of water, maintain the temperature at
50 DEG C, PH 5.0, after carrying out enzymolysis processing 1h, add 0.7% cellulase and pectase (1.5 of bulk drug weight:1),
It is put into after digesting 1h again in water distillation apparatus device, carries out steam distillation extraction 4h, collect volatile oil；
(2) continuous dynamic concentration of alcohol extraction
The Ligusticum wallichii of recipe quantity, aconiti preparata,radix, pyritum ignited, No. four copper powders are ground into coarse powder to mix, cross 40 mesh scalpings, are merged
The dregs of a decoction in step (1), material is put into from the dog-house of extractor, and after feeding intake, 4 times of amounts are added in Chinese medicament extracting device
95% ethanol solution, heating stirring is carried out to extractor, and it is 70 DEG C to control final temperature；One water of connection at the top of extractor
Case, it is allowed to connect with extractor, valve switch and flowmeter is provided between water tank and extractor, wherein flowmeter can controls water
Water flows into the speed of extractor in case；While being heated to extractor, also water in water tank is heated, made in water tank
Water temperature is consistent with temperature in extractor；
After temperature stabilization in water tank and extractor, the valve switch of water tank is opened, water velocity is adjusted, makes ethanol dense
Degree rate of change is 0.75%/min, reacts 60min, concentration of alcohol is reached 50%, after first set reaction terminates, and collects extraction
Liquid；The step of ethanol that 3 times of amount concentration are 50% is added in the dregs of a decoction after first set reaction terminates, and is reacted according to first is delayed
Slow plus water, it is 0.45%/min to make concentration of alcohol rate of change, reacts 88min, concentration of alcohol is reached 10.4%；Collect filtrate,
The filtrate collected after cold filtration with first time merges, and obtains extract solution；
(3) vacuum-concentrcted
When using the vacuum-concentrcted technique to be condensed into 60 DEG C the extract solution in step (2) relative density for 1.26 it is thick
Cream, 60 DEG C be dried under reduced pressure after be ground into dry extract, cross 14 mesh sieves；
(4) preparation of tablet
Dry extract and volatile oil obtained above are taken, adds appropriate talcum powder and microcrystalline cellulose (2:1), carboxymethyl forms sediment
Powder sodium, it is well mixed, through softwood processed, pelletizes, dry, is pressed into 400, film coating, every 0.62g.
Embodiment 3
Preparation method：
(1) extraction of volatile oil
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder after mixing, cross 40 mesh sieves, first
Secondary plus bulk drug weight 0.5% cellulase and pectase (1.5:1), stir, add 8 times of water, maintain the temperature at
45 DEG C, PH 4.5, after carrying out enzymolysis processing 1h, add 0.7% cellulase and pectase (1.5 of bulk drug weight:1),
It is put into after digesting 1h again in water distillation apparatus device, carries out steam distillation extraction 6h, collect volatile oil；
(2) continuous dynamic concentration of alcohol extraction
The Ligusticum wallichii of recipe quantity, aconiti preparata,radix, pyritum ignited, No. four copper powders are ground into coarse powder to mix, cross 40 mesh scalpings, are merged
The dregs of a decoction in step (1), material is put into from the dog-house of extractor, and after feeding intake, 4 times of amounts are added in Chinese medicament extracting device
95% ethanol solution, heating stirring is carried out to extractor, and it is 65 DEG C to control final temperature；One water of connection at the top of extractor
Case, it is allowed to connect with extractor, valve switch and flowmeter is provided between water tank and extractor, wherein flowmeter can controls water
Water flows into the speed of extractor in case；While being heated to extractor, also water in water tank is heated, made in water tank
Water temperature is consistent with temperature in extractor；
After temperature stabilization in water tank and extractor, the valve switch of water tank is opened, water velocity is adjusted, makes ethanol dense
Degree rate of change is 0.8%/min, reacts 56min, concentration of alcohol is reached 50%, after first set reaction terminates, and collects extract solution；
The step of ethanol that 3 times of amount concentration are 50% is added in the dregs of a decoction after first set reaction terminates, and is reacted according to first is slowly
Add water, it is 0.5%/min to make concentration of alcohol rate of change, reacts 80min, concentration of alcohol is reached 10%；Filtrate is collected, it is cooled
The filtrate collected after filter with first time merges, and obtains extract solution；
(3) vacuum-concentrcted
When using the vacuum-concentrcted technique to be condensed into 60 DEG C the extract solution in step (2) relative density for 1.25 it is thick
Cream, 60 DEG C be dried under reduced pressure after be ground into dry extract, cross 14 mesh sieves；
(4) preparation of tablet
Dry extract and volatile oil obtained above are taken, adds appropriate talcum powder and microcrystalline cellulose (2:1), carboxymethyl forms sediment
Powder sodium, it is well mixed, through softwood processed, pelletizes, dry, is pressed into 400, film coating, every 0.62g.
Embodiment 4
Preparation method：
(1) extraction of volatile oil
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder after mixing, cross 40 mesh sieves, first
Secondary plus bulk drug weight 0.5% cellulase and pectase (1.5:1), stir, add 10 times of water, maintain the temperature at
60 DEG C, PH 5.5, after carrying out enzymolysis processing 1h, add 0.7% cellulase and pectase (1.5 of bulk drug weight:1),
It is put into after digesting 1h again in water distillation apparatus device, carries out steam distillation extraction 5h, collect volatile oil；
(2) continuous dynamic concentration of alcohol extraction
The Ligusticum wallichii of recipe quantity, aconiti preparata,radix, pyritum ignited, No. four copper powders are ground into coarse powder to mix, cross 40 mesh scalpings, are merged
The dregs of a decoction in step (1), material is put into from the dog-house of extractor, and after feeding intake, 3 times of amounts are added in Chinese medicament extracting device
95% ethanol solution, heating stirring is carried out to extractor, and it is 70 DEG C to control final temperature；One water of connection at the top of extractor
Case, it is allowed to connect with extractor, valve switch and flowmeter is provided between water tank and extractor, wherein flowmeter can controls water
Water flows into the speed of extractor in case；While being heated to extractor, also water in water tank is heated, made in water tank
Water temperature is consistent with temperature in extractor；
After temperature stabilization in water tank and extractor, the valve switch of water tank is opened, water velocity is adjusted, makes ethanol dense
Degree rate of change is 0.9%/min, reacts 50min, concentration of alcohol is reached 50%, after first set reaction terminates, and collects extract solution；
The step of ethanol that 4 times of amount concentration are 50% is added in the dregs of a decoction after first set reaction terminates, and is reacted according to first is slowly
Add water, it is 0.4%/min to make concentration of alcohol rate of change, reacts 100min, concentration of alcohol is reached 10%；Collect filtrate, cooling
The filtrate collected after filtering with first time merges, and obtains extract solution；
(3) vacuum-concentrcted
When using the vacuum-concentrcted technique to be condensed into 60 DEG C the extract solution in step (2) relative density for 1.26 it is thick
Cream, 60 DEG C be dried under reduced pressure after be ground into dry extract, cross 14 mesh sieves；
(4) preparation of tablet
Dry extract and volatile oil obtained above are taken, adds appropriate talcum powder and microcrystalline cellulose (2:1), carboxymethyl forms sediment
Powder sodium, it is well mixed, through softwood processed, pelletizes, dry, is pressed into 400, film coating, every 0.62g.
Comparative example 1
Preparation method：
(1) take No. four copper powders, aconiti preparata,radix, vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, pyritum ignited to be ground into fine powder, sieve, mix；
(2) Ligusticum wallichii, Radix Angelicae Sinensis are taken, with 70% ethanol as solvent, is percolated, filtrate recycling ethanol, is concentrated under reduced pressure into cream；
(3) above-mentioned fine powder and auxiliary material are added, is mixed, is made particle, less than 60 DEG C dryings are pressed into 1000, sugar coating,
Produce.
Comparative example 2
Preparation method：
(1) Ligusticum wallichii, Radix Angelicae Sinensis, vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar is taken to be added to supercritical CO2In extractor, ethanol is as entrainment
Agent, extracting pressure 20Mpa, 40 DEG C of temperature, CO2Flow 2m1/g crude drug min, extraction time 160min, obtain supercritical extract
Thing, it is standby；
(2) take aconiti preparata,radix, pyritum ignited, No. four copper powders to crush, add 2L 70% ethanol, put into microwave extracting apparatus
Microwave abstracting is carried out, extracts power 500W, is extracted 2 times, each 6min, combining extraction liquid, concentration, is added to D102 macroporous absorption trees
On fat, 50% ethanol elutions, 5 times of amount column volume eluents are collected, ethanol is recovered under reduced pressure, is concentrated and dried, obtains Microwave Extraction thing,
It is standby；
(3) above-mentioned supercritical extract and Microwave Extraction thing are mixed, adds starch, the pelleting of 70% ethanol, dry, pressure
Piece, it is made 1000.
Comparative example 3
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder, cross 40 mesh sieves, add 8 times of amounts
Water, 4h is distilled, collect volatile oil.
Comparative example 4
By the raw material recipe quantity in step (2) in embodiment 1, the alcohol reflux for adding 90% extracts 2 times, 2 hours every time,
70 DEG C of Extracting temperature, merge filtrate twice, obtain extract solution.
Comparative example 5
By the raw material recipe quantity in step (2) in embodiment 1, the alcohol reflux for adding 50% extracts 2 times, 2 hours every time,
70 DEG C of Extracting temperature, merge filtrate twice, obtain extract solution.
The research of preparation technology in each step of this product of experimental example 1
The research of 1.1 Extraction Process of Volatile Oil
Using the extraction that vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis are carried out to volatile oil in this product preparation process (1), use
Enzymolysis pre-treatment is first carried out, strengthens the extraction of volatile oil, the influence factor of enzyme class is investigated, the results are shown in Table 1.
1.1.1 the investigation of enzyme class
Influence of the 1 different enzymes of table to extraction process
| Enzyme class | Oil yield of volatilizing (%) |
| Protease | 2.64 |
| Pectase | 2.85 |
| Cellulase | 2.92 |
| Cellulase and pectase 1：1 | 3.12 |
| Cellulase and pectase 1.5：1 | 3.21 |
| Cellulase and pectase 2：1 | 3.01 |
Test result indicates that：Selection carries out enzymolysis pre-treatment with cellulase and this complex enzyme of pectase, is more beneficial for
The extraction of volatile oil.
1.1.2 the technique of different disposal extraction volatile oil is investigated
The extraction of volatile oil is carried out under optimal enzymatic hydrolysis condition, and with not carrying out the steam distillation method ratio of ferment treatment
Compared with as a result such as table 2 below.
The different disposal of table 2 extracts volatile oil results contrast
As shown in Table 2, digest compared with traditional extraction technique, extraction is abundant, efficiency high.Its main cause may be compound
Enzymolysis process destroys plant cell wall, is advantageous to the extraction of active ingredient, can improve oil yield.
The research of 1.2 continuous dynamic concentration of alcohol extraction processes
Chemical composition of Chinese materia medica is complicated, and heterogeneity polarity difference is big, such as the polyhydroxy that glucose, sucrose equimolecular are smaller
Based compound, there is strongly hydrophilic, be highly soluble in water.Protein and amino acid are all soda acid amphoteric compounds, are had to a certain degree
Polarity, so water can be dissolved in, do not dissolve in or the sub- organic solvent of indissoluble.The solubility of flavone compound is because of structure and shape be present
State (glycosides or aglycon, monoglycosides, disaccharide glycosides or three glucosides) is different and has very big difference.Glycoside is all stronger than the hydrophily of its aglycon,
Particularly for saponin(e due to being often combined with most glycan molecules in their molecule, hydroxy number is more, can show stronger hydrophilic
Property, and sapogenin then belongs to the strong compound of lipophilicity.The free alkaloid of majority is lipophilic compound, and salt is combined into acid
Afterwards, it can ionize, strengthen polarity, these alkaloids can be described as semi-polarity compound.So the salt of alkaloid is soluble in
Water, it is insoluble or be insoluble in organic solvent；And most free alkaloids is insoluble or is insoluble in water, lipophilic solvent is soluble in.Oil
Fat, volatile oil, fat-soluble pigment are all strong lipophilic compositions.Traditional Chinese medicine extraction generally require it is as much as possible extraction effectively into
Point, strengthen pharmaceutical activity.The present invention can be extracted more fully using the method extraction Chinese medicine of continuous dynamic concentration of alcohol extraction
The active ingredient of opposed polarity.
Content assaying method is as follows：
(1) Determination Method of Flavone Content
Determination of total flavonoids presses 2010 editions《Pharmacopoeia of People's Republic of China》The A ultraviolet spectrophotometries of (one) annex V
Carried out under to Determination of Total Flavonoids.
(2) content assaying method of forulic acid
Chromatographic condition is as follows：Using the strong silica gel that closes of octadecylsilane as filler, mobile phase is the phosphoric acid of acetonitrile -0.085%
Solution (17:83)；Flow velocity：1mL·min-1；Detection wavelength：316nm；Column temperature：35℃；Sample size：10μl.
The medicinal extract 0.5g for taking said extracted technique to prepare, 70% ethanol dissolves constant volume in volumetric flask, then uses miillpore filter
After (0.45 μm) filtering, inject in high performance liquid chromatograph, quantified by external standard method is carried out with forulic acid reference substance, measures forulic acid
Content.It the results are shown in Table 3.
The comparison of the present invention of table 3 extraction result and existing process
| Embodiment is numbered | General flavone content (%) | Ferulaic acid content (%) |
| Embodiment 1 | 5.23 | 0.80 |
| Embodiment 2 | 4.98 | 0.84 |
| Embodiment 3 | 5.01 | 0.82 |
| Embodiment 4 | 5.25 | 0.87 |
| Comparative example 1 | 2.67 | 0.49 |
| Comparative example 2 | 3.24 | 0.64 |
| Comparative example 4 | 3.78 | 0.58 |
| Comparative example 5 | 3.89 | 0.61 |
By relatively, compared with traditional extraction process, being extracted using the method for continuous dynamic concentration of alcohol extraction
Comparison of ingredients is complete, extracts active ingredients efficiency high.
The research of 1.3 tablet for curing fracture granulating process
1.3.1 the selection of filler species
(1) measure of fine powder rate：By the particle of whole grain about 10g, sieved with 60 mesh sieves, fine powder rate is calculated as follows：Carefully
Powder rate=pass through 60 mesh sieve fine powders/total number of particles × 100%.
(2) measure of Moisture percentage：Dry granule is placed in the measuring cup bottom of constant temperature, it is accurate to tile
It is placed in after weighing in the drier of sodium chloride supersaturated solution, 6h is preserved in 40 DEG C of insulating boxs and is weighed, moisture absorption is calculated as follows
Percentage：Weight × 100% before Moisture percentage (%)=(weight before weight-moisture absorption after moisture absorption)/moisture absorption.
Dry extract and various types of filler is taken to be well mixed in 3: 1 ratios, the granulation of the mesh of 70% ethanol 30,80 DEG C of dryings,
20 mesh sieve whole grains are crossed, gained particle carries out fine powder rate and Moisture percentage measure, and observes particle appearance, hardness, particle effect
Situation.It the results are shown in Table 4.
The effect expedition of the filler of table 4
1.3.2 the selection of disintegrant species
By thick paste produced by the present invention, dried starch, sodium carboxymethyl starch, PVPP, low-substituted hydroxypropyl are separately added into
Base cellulose, investigates disintegration time limited respectively.It the results are shown in Table 5.
The effect expedition of the disintegrant of table 5
| Disintegrant species | Disintegration time limited (min) |
| Dried starch | 10 |
| Sodium carboxymethyl starch | 6 |
| PVPP | 8 |
| Low-substituted hydroxypropyl cellulose | 9 |
Test result indicates that the disintegration from sodium carboxymethyl starch is most fast.Sodium carboxymethyl starch water suction after powder expansion and
It is insoluble, colloidal solution is not formed, therefore continuing infiltration and influenceing the further disintegration of tablet for moisture is not hindered, it is auxiliary with respect to other
Material is more suitable for the disintegrant of full medicinal extract piece.
Experimental example 2
Experiment material：
Kunming mouse, body weight 18-22g, 70；Standard Wistar rats, body weight 180-200g, 140.
2.1 analgesic effect
Above-mentioned mouse is taken, 7 groups are randomly divided into by body weight, every group 10, wherein 6 groups of difference gastric infusions, dosage are
2.0g/kg, blank control group give the distilled water of equivalent, once a day, successive administration 10 days, the injection of last dose 1h pneumoretroperitoneums
0.7% acetic acid 0.1mg/g.Writhing response number caused by each group animal oil acetic acid in 15 minutes is observed, the results are shown in Table 6.
Influence of the tablet for curing fracture of table 6 to mouse analgesic effect
| Group | n | Dosage (g/kg) | Writhing number |
| Blank control group | 10 | - | 38.2±2.3 |
| Tablet group (commercially available) | 10 | 2.0 | 12.5±4.2** |
| Comparative example 1 | 10 | 2.0 | 14.3±4.3** |
| Embodiment 1 | 10 | 2.0 | 9.4±3.6** |
| Embodiment 2 | 10 | 2.0 | 9.8±3.1** |
| Embodiment 3 | 10 | 2.0 | 10.1±3.2** |
| Embodiment 4 | 10 | 2.0 | 9.2±2.8** |
Note：Compared with blank control group, * P<0.05, * * P<0.01
As a result show：The writhing number of the tablet group of the present invention is considerably less than blank control group (p<0.01), Dichlorodiphenyl Acetate institute
Mouse writhing reaction is caused to have obvious inhibiting effect, the medical instrument has obvious analgesic activity.
Effect of 2.2 tablet for curing fracture to ecchymosis
Above-mentioned rat is taken, 7 groups is randomly divided into, every group 10, removes rat back mouse hair, 5* within 18 hours before experiment
4cm2, with this epilating area of mouse clamp, cause subcutaneous hemorrhage.After 12h, by 2.0g/kg, wherein gastric infusion, blank control
Group gives the distilled water of equivalent.It is administered daily 1 time, successive administration 7 days, visually observes swelling and ecchymosis regression situation during administration,
Residual area is measured, is scored, to its total score as ecchymosis severity, the results are shown in Table 8.
The standards of grading of the ecchymosis of table 7
The influence that the tablet for curing fracture of table 8 is acted on mouse ecchymosis
Note：Compared with blank control group, * P<0.05, * * P<0.01
As a result show：Diffusion of the tablet group of the present invention to ecchymosis also has the effect of obvious.
Influence of 2.3 tablet for curing fracture to hemorheology of rat
Above-mentioned rat 70 is taken, male and female dual-purpose, 7 groups is randomly divided into, every group 10, uses 8%Na within 24 hours before experiment2S
Remove rat back mouse hair, 5 × 4cm2.By 2.0g/kg, gastric infusion, wherein blank control group give the distilled water of equivalent.Often
Day is administered once, successive administration 7 days, after last time is administered 1 hour, plucks rat eye and takes blood, surveys WBV, whole blood reduction
Viscosity content.Then statistical analysis, 9 be the results are shown in Table.
Influence of the tablet for curing fracture of table 9 to hemorheology of rat
Note：Compared with blank control group, * P<0.05, * * P<0.01
As a result show：Tablet for curing fracture can significantly reduce whole blood viscosity and Plasma Viscosity, improve hemorheological property, make fracture site
Blood supply be improved significantly, accelerate absorption of hematoma, promote proliferation of fibrous tissue, fiber poroma, which is formed, to be accelerated.
Claims (2)
1. a kind of tablet for curing fracture, its prescription includes Radix Angelicae Sinensis 39g, vinegar stir-baked OLIBANUM 39g, vinegar stir-baked MYRRHA with vinegar 39g, aconiti preparata,radix 39g, Ligusticum wallichii 39g,
Pyritum ignited 39g, No. four copper powder 2.34g；It is characterized in that：The preparation method of the tablet for curing fracture comprises the following steps：
(1) extraction of volatile oil
Take the vinegar stir-baked OLIBANUM, vinegar stir-baked MYRRHA with vinegar, Radix Angelicae Sinensis bulk drug of recipe quantity to be ground into coarse powder after mixing, cross 40 mesh sieves, add for the first time
0.5% proportioning of bulk drug weight is 1.5:1 cellulase and pectase, stirs, and adds 6-10 times of water, keeps temperature
Degree is at 40 DEG C -60 DEG C, PH 4.0-5.5, and after carrying out enzymolysis processing 1h, 0.7% proportioning for adding bulk drug weight is 1.5:1
Cellulase and pectase, then be put into after digesting 1h in water distillation apparatus device, carry out steam distillation extraction 4-6h, collection is waved
Hair oil；
(2) continuous dynamic concentration of alcohol extraction
The Ligusticum wallichii of recipe quantity, aconiti preparata,radix, pyritum ignited, No. four copper powders are ground into coarse powder to mix, cross 40 mesh scalpings, combining step
(1) dregs of a decoction in, material is put into from the dog-house of extractor, after feeding intake, 95% second is added in Chinese medicament extracting device
Alcoholic solution, heating stirring is carried out to extractor, and it is 60 DEG C -75 DEG C to control final temperature；One water tank of connection, makes at the top of extractor
Connected with extractor, valve switch and flowmeter are provided between water tank and extractor, wherein flowmeter can be controlled in water tank
Water flows into the speed of extractor；While being heated to extractor, also water in water tank is heated, makes Water in Water Tanks temperature
It is consistent with temperature in extractor；
After temperature stabilization in water tank and extractor, the valve switch of water tank is opened, water velocity is adjusted, changes concentration of alcohol
Rate is 0.75%-0.9%/min, reacts 50min-60min, after first set reaction terminates, collects extract solution；In first set reaction
The step of 50% ethanol is added in the dregs of a decoction after end, and is reacted according to first slowly adds water, makes the concentration of alcohol rate of change be
0.4%-0.5%/min, react 80min-100min；Filtrate is collected, the filtrate collected after cold filtration with first time merges, obtained
Extract solution；
(3) vacuum-concentrcted
Relative density is 1.25-1.26's when using the vacuum-concentrcted technique to be condensed into 60 DEG C the extract solution in step (2)
Thick paste, 60 DEG C be dried under reduced pressure after be ground into dry extract, cross 14 mesh sieves；
(4) preparation of tablet
Dry extract and volatile oil are taken, adds appropriate filler, disintegrant, is well mixed, through softwood processed, dries, pelletizes, compacting
Into 400, film coating, every 0.62g, wherein, the filler is selected from microcrystalline cellulose and talcum powder；The disintegrant choosing
From sodium carboxymethyl starch.
2. tablet for curing fracture according to claim 1, it is characterised in that：Continuous dynamic concentration of alcohol carries for the first time in step (2)
It is 70 DEG C to take temperature, and addition is 3 times of 95% ethanol, concentration of alcohol rate of change 0.9%/min, extraction time 50min, the
Second extraction temperature is 70 DEG C, and addition is 4 times of 50% ethanol, and concentration of alcohol rate of change is 0.4%/min, and extraction time is
100min。
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|---|---|---|---|---|
| CN1359671A (en) * | 2000-12-18 | 2002-07-24 | 孙庆寿 | Process for preparing tablet for quickly setting up bone |
| CN1403111A (en) * | 2002-03-15 | 2003-03-19 | 通化正和药业有限公司 | Bone-setting medicine |
| CN102359992A (en) * | 2011-08-26 | 2012-02-22 | 通化正和药业有限公司 | Bone-setting tablet, method thereof for identifying and measuring content |
| CN102988509A (en) * | 2012-10-15 | 2013-03-27 | 李正梅 | Preparation method and application of bone-knitting tablet |
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| CN1359671A (en) * | 2000-12-18 | 2002-07-24 | 孙庆寿 | Process for preparing tablet for quickly setting up bone |
| CN1403111A (en) * | 2002-03-15 | 2003-03-19 | 通化正和药业有限公司 | Bone-setting medicine |
| CN102359992A (en) * | 2011-08-26 | 2012-02-22 | 通化正和药业有限公司 | Bone-setting tablet, method thereof for identifying and measuring content |
| CN102988509A (en) * | 2012-10-15 | 2013-03-27 | 李正梅 | Preparation method and application of bone-knitting tablet |
| CN104856968A (en) * | 2015-05-27 | 2015-08-26 | 韩志强 | Traditional Chinese medicine tablet with effects of removing thrombus and dredging collaterals and preparation method thereof |
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